CN115651519A - Composite hydrogen permeation resistant coating for hydrogen transmission pipeline and preparation method thereof - Google Patents
Composite hydrogen permeation resistant coating for hydrogen transmission pipeline and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a composite hydrogen permeation resistant coating for a hydrogen transmission pipeline and a preparation method thereof, wherein the coating comprises the following components: the bottom layer is a molybdenum disulfide coating, and the surface layer is a modified fluorine-containing coating. The preparation method comprises the following steps: uniformly mixing molybdenum disulfide powder and a dispersant to obtain a component A; adding a binder into the component A, stirring, and heating in vacuum to obtain a component B; melting the component B into a diluent and adding a curing agent to obtain a molybdenum dioxide coating; spraying the molybdenum dioxide coating on the surface of the hydrogen pipeline substrate, and preserving heat after spraying; modifying the fluorine-containing coating by adopting graphene oxide to obtain a modified fluorine-containing coating; and after the bottom layer is completely dried, spraying the modified fluorine-containing coating on the surface of the bottom layer, and finally baking to form a stable surface layer. The invention can effectively prolong the service life of the hydrogen conveying pipeline and improve the safety of the pipeline operation.
Description
Technical Field
The invention belongs to the technical field of pipeline steel surface modification, and particularly relates to a composite hydrogen permeation resistant coating for a hydrogen transmission pipeline and a preparation method thereof.
Background
The global energy demand is on an increasing trend, and overuse of fossil fuels not only depletes existing non-renewable resources, but also poses serious environmental problems. Renewable energy sources such as solar, wind, tidal/wave and nuclear have received some attention as alternatives to fossil energy sources, but their practical use remains limited due to their intermittent and unpredictable nature. Hydrogen energy is one of the cleanest energy sources, and is becoming the first choice for replacing non-renewable energy sources due to its high energy conversion efficiency and environmental protection characteristics. The storage and transportation of hydrogen energy is an important link in the development of hydrogen energy industry, the safe operation of a hydrogen transportation pipeline faces a severe challenge, and the problem of pipeline steel failure caused by hydrogen embrittlement draws wide attention. Hydrogen embrittlement refers to interaction of hydrogen entering into metal and a matrix, so that mechanical properties of the material are damaged, and further phenomena such as bubbling and cracking are generated.
The pipeline steel is a common material for hydrogen conveying pipelines, and is commonly X42, X52, X56, X70, X80 and the like. Covering the surface with a coating with the function of delaying hydrogen permeation is one of important means for solving the problem of hydrogen embrittlement of steel. The design of the coating for delaying the hydrogen permeation mainly takes two aspects into consideration, on one hand, the coating with low porosity and high density is prepared to block the hydrogen from entering; on the other hand, multiple hydrogen traps are made to trap hydrogen atoms, thereby reducing the concentration of free hydrogen that can diffuse in the material.
Most of the conventional hydrogen permeation resistant coatings are metal oxide coatings, silicide coatings, aluminide coatings and the like; the preparation process also has certain differences, such as chemical/physical vapor deposition method, plasma spraying method, sol-gel method, micro-arc oxidation method and the like. The preparation process and conditions are complex, the cost is high, and the requirements of large-scale and long-distance pipeline steel use cannot be met; in addition, the inorganic ceramic coating is relatively brittle and easy to crack, which has certain limitation in practical application. The practical application of the pipeline steel coating not only needs to consider the hydrogen permeation resistance, but also needs to consider the corrosion resistance, which puts higher requirements on the component and the structural design of the coating. Therefore, the invention of the novel composite hydrogen permeation resistant coating for the pipeline steel is of great importance in the aspects of prolonging the service life of the pipeline steel, expanding the industrial application and the like.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a novel composite hydrogen permeation resistant coating for a hydrogen transmission pipeline and a preparation method thereof.
The invention is realized by the following technical scheme.
A composite hydrogen permeation resistant coating for a hydrogen transmission pipeline, the coating comprising: the bottom layer is a molybdenum disulfide coating, and the surface layer is a modified fluorine-containing coating.
Further, the modified fluorine-containing coating is one or more of a modified polytetrafluoroethylene coating, a polyvinylidene fluoride coating and a fluorine-silicon coating.
Further, the solid content of the molybdenum disulfide in the bottom layer is 38% -60%.
Furthermore, the thickness of the bottom layer is 20-80 μm, the thickness of the surface layer is 60-150 μm, and the total thickness of the composite hydrogen permeation resistant coating is 80-230 μm.
Further, the hydrogen conveying pipeline is pipeline steel.
A preparation method of a composite hydrogen permeation resistant coating for a hydrogen transmission pipeline comprises the following steps:
(1) Preparation of the bottom layer: uniformly mixing molybdenum disulfide powder and a dispersing agent, and ultrasonically mixing and stirring for 20-60min to obtain a component A; adding a binder into the component A, uniformly stirring at the rotating speed of 600-1200r/min, heating to 55-80 ℃ in vacuum, and preserving heat for 60-300min to obtain a component B; the component B is blended into a diluent and added with a curing agent, and the mixture is uniformly stirred at the rotating speed of 800-1500r/min to obtain a molybdenum dioxide coating; spraying the molybdenum dioxide coating on the surface of the hydrogen conveying pipeline substrate, and keeping the temperature at 160-250 ℃ for 20-90min after spraying;
(2) Preparation of the surface layer: modifying the fluorine-containing coating by using graphene oxide, wherein the addition amount of the graphene oxide is 0.1-5%, and the dispersion is carried out for 10-60min at the rotating speed of 800-1500r/min to obtain the modified fluorine-containing coating; and (2) after the bottom layer prepared in the step (1) is completely dried, spraying the modified fluorine-containing coating on the surface of the bottom layer, and finally baking to form a stable surface layer.
Further, the diameter of the molybdenum disulfide powder in the step (1) is 100-800nm; the weight ratio of the molybdenum disulfide powder to the dispersant is 1:10-20 percent, the addition amount of the binder is 30-60 percent of the weight of the component A, and the mass ratio of the addition amount of the diluent to the component B is (1-3): 1, the addition amount of the curing agent is 10-30% of the weight of the binder.
Further, the dispersing agent is one of acetone or ethanol solution containing 0.1-5% of silane coupling agent, the binder is thermosetting polyurethane, the diluent is water, and the curing agent is isocyanate.
Further, before the molybdenum dioxide coating is sprayed on the surface of the hydrogen conveying pipeline substrate in the step (1), the surface rust and the oxidation film are removed by polishing with coarse-to-fine sand paper, and oil removal and drying treatment are carried out.
Furthermore, the preparation process and the spraying process of the bottom layer and the surface layer are that the coating is put into high-pressure airless spraying equipment and is sprayed under the high pressure of 10-20 Mpa.
Further, the fluorine-containing coating in the step (2) is one or more of polytetrafluoroethylene, polyvinylidene fluoride and fluorine silicon.
Further, in the preparation process of the surface layer in the step (2), the baking process is carried out in a muffle furnace at the temperature of 150-300 ℃, and the surface layer is taken out and placed at room temperature after heat preservation for 20-90 min.
The composite hydrogen permeation resistant coating for the hydrogen transmission pipeline provided by the invention has the beneficial technical effects that the composite hydrogen permeation resistant coating is an inorganic and organic composite coating, wherein molybdenum disulfide is used as a novel lamellar material, has a special crystal structure and stronger hydrogen permeation resistance, can stably exist at a temperature below 500 ℃ and does not react with hydrogen, and has the potential of being used as a novel hydrogen blocking layer.
Polytetrafluoroethylene coatings, polyvinylidene fluoride coatings, fluorosilicone coatings and the like are commonly used in the fields of protection of buildings or corrosion prevention of metals. The graphene oxide is also used as a two-dimensional material and is easy to combine with hydrogen, when the hydrogen atoms are very close to the graphene, the C-H bond can be formed only by the energy of 0.18eV, and the graphene oxide has very strong capture capacity on the hydrogen; meanwhile, pi bonds in the graphene oxide form dense electron cloud distribution, so that strong repulsive force is provided for tunneling particles, and the graphene oxide has a high energy barrier for tunneling of hydrogen atoms. That is to say, the graphene oxide remarkably increases the difficulty of hydrogen permeation, prolongs the hydrogen permeation path, and can remarkably improve the hydrogen resistance of the coating; on the other hand, the graphene oxide remarkably improves the corrosion resistance of the composite coating, which is also necessary under the actual working conditions in the pipeline.
The invention integrates the advantages of each layer, can effectively prolong the service life of the hydrogen transmission pipeline in the development process of the hydrogen energy industry, can effectively solve the waste and pollution caused by hydrogen permeation in energy application, and improves the safety of pipeline operation.
Drawings
FIG. 1 is an electrochemical hydrogen permeation curve of example 1;
FIG. 2 is an electrochemical hydrogen permeation curve of example 2;
FIG. 3 is an electrochemical hydrogen permeation curve of example 3;
fig. 4 is SEM images before and after the electrochemical hydrogen permeation performance test of comparative example 1.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
Example 1
Selecting an X80 pipeline steel base material with the size of 30mm 1mm, sequentially polishing the surface by 600#, 800#, 1000#, and 1200# abrasive paper, sequentially ultrasonically cleaning in deionized water, ethanol and acetone to remove an oxide film and rust on the surface, naturally drying, and standing for later use.
According to the weight ratio of 1: weighing molybdenum disulfide powder and an acetone solution containing 1% of silane coupling agent according to the proportion of 10, uniformly mixing, and ultrasonically mixing and stirring for 30min to obtain a component A; adding thermosetting polyurethane which is half the weight of the component A as a binder, uniformly stirring at the rotating speed of 1000r/min, heating to 65 ℃ in vacuum, and preserving heat for 200min to obtain a component B. And (3) melting the component B into water with the same mass, adding isocyanate with the weight being 20% of that of the binder, and uniformly stirring at the rotating speed of 1500r/min to obtain the molybdenum disulfide coating. Spraying molybdenum disulfide coating on the surface of the X80 matrix, and keeping the temperature at 250 ℃ for 60min after spraying. The sample was taken out and cooled to room temperature, and the thickness was 60 μm. The spraying process is to load the molybdenum disulfide coating into high-pressure airless spraying equipment and spray the molybdenum disulfide coating through high pressure of 10 Mpa. Wherein the diameter of the molybdenum disulfide powder is 100nm, and the solid content of the molybdenum disulfide in the bottom layer is 45%;
and dispersing 1% of graphene oxide in the slurry of the polyvinylidene fluoride by mass, and stirring at the rotating speed of 1500r/min for 30min to obtain the modified slurry of the polyvinylidene fluoride.
After the bottom layer was completely dried, a slurry of modified polyvinylidene fluoride was sprayed and baked in a muffle furnace at 230 ℃ for 30min to obtain a surface layer having a thickness of 100 μm. Wherein the spraying process comprises the steps of filling the slurry of the modified polyvinylidene fluoride into high-pressure airless spraying equipment, and spraying at a high pressure of 10 Mpa.
Example 2
Selecting an X80 pipeline steel base material with the size of 30mm 1mm, sequentially polishing the surface by 600#, 800#, 1000# and 1200# abrasive paper, sequentially carrying out ultrasonic cleaning in deionized water, ethanol and acetone to remove an oxide film and rust on the surface, naturally air-drying, and standing for later use.
According to the weight ratio of 1: weighing molybdenum disulfide powder and an acetone solution containing 3% of silane coupling agent according to the proportion of 20, uniformly mixing, and carrying out ultrasonic mixing and stirring for 20min to obtain a component A; adding thermosetting polyurethane accounting for 40% of the weight of the component A as a binder, uniformly stirring at the rotating speed of 800r/min, heating to 70 ℃ in vacuum, and preserving heat for 100min to obtain a component B. And (2) melting the component B into water according to the mass ratio of 2. The preparation method is characterized in that the preparation method is adopted for preparing the X80 matrix surface in a spraying mode, and the temperature is kept for 60min at 160 ℃ after the spraying. The substrate was taken out and cooled to room temperature to prepare a bottom layer having a thickness of 70 μm. The spraying process is to load the molybdenum disulfide coating into high-pressure airless spraying equipment and spray the molybdenum disulfide coating at the high pressure of 18 Mpa. Wherein the diameter of the molybdenum disulfide powder is 300nm, and the solid content of the molybdenum disulfide in the bottom layer is 52%.
And dispersing graphene oxide with the mass ratio of 0.5% in the slurry of the polyvinylidene fluoride, and stirring at the rotating speed of 1200r/min for 60min to obtain the modified slurry of the polyvinylidene fluoride.
After the bottom layer was completely dried, a slurry of modified polyvinylidene fluoride was sprayed and baked in a muffle furnace at 200 ℃ for 30min to obtain a surface layer having a thickness of 95 μm. Wherein the spraying process comprises the steps of filling the slurry of the modified polyvinylidene fluoride into high-pressure airless spraying equipment, and spraying at the high pressure of 18 Mpa.
Example 3
Selecting an X80 pipeline steel base material with the size of 30mm 1mm, sequentially polishing the surface by 600#, 800#, 1000# and 1200# abrasive paper, sequentially carrying out ultrasonic cleaning in deionized water, ethanol and acetone to remove an oxide film and rust on the surface, naturally air-drying, and standing for later use.
According to the weight ratio of 1:10, weighing molybdenum disulfide powder and an ethanol solution containing 1% of silane coupling agent according to the proportion, uniformly mixing, and carrying out ultrasonic mixing and stirring for 40min to obtain a component A; adding 30 percent of thermosetting polyurethane of the weight of the component A as a binder, stirring uniformly at the rotating speed of 1200r/min, heating to 70 ℃ in vacuum, and preserving heat for 150min to obtain a component B. And (3) melting the component B into water according to the mass ratio of 3. The preparation method is characterized in that the preparation method is adopted for preparing the X80 matrix surface in a spraying mode, and the temperature is kept for 60min at 210 ℃ after the spraying. The sample was taken out and cooled to room temperature, and the thickness was 65 μm. The spraying process is to load the molybdenum disulfide coating into high-pressure airless spraying equipment and spray the molybdenum disulfide coating through high pressure of 15 Mpa. Wherein the diameter of the molybdenum disulfide powder is 500nm, and the solid content of the molybdenum disulfide in the bottom layer is 40%.
And dispersing the graphene oxide with the mass ratio of 3% in the slurry of the fluorine silicon, and stirring at the rotating speed of 950r/min for 20min to obtain the modified slurry of the fluorine silicon.
And after the bottom layer is completely dried, spraying modified fluorosilicone slurry, and baking in a muffle furnace at 150 ℃ for 50min to obtain the surface layer with the thickness of 90 mu m. Wherein the spraying process comprises the steps of loading the slurry of the modified fluorine silicon into high-pressure airless spraying equipment, and spraying at a high pressure of 15 Mpa.
Example 4
Selecting an X80 pipeline steel base material with the size of 30mm 1mm, sequentially polishing the surface by 600#, 800#, 1000# and 1200# abrasive paper, sequentially carrying out ultrasonic cleaning in deionized water, ethanol and acetone to remove an oxide film and rust on the surface, naturally air-drying, and standing for later use.
1:15, weighing molybdenum disulfide powder and an ethanol solution containing 1% of silane coupling agent, uniformly mixing, and ultrasonically mixing and stirring for 60min to obtain a component A; adding thermosetting polyurethane which accounts for 60% of the weight of the component A as a binder, uniformly stirring at the rotating speed of 1200r/min, heating to 80 ℃ in vacuum, and preserving heat for 200min to obtain a component B. And (3) melting the component B into water with the same mass, adding isocyanate accounting for 30% of the weight of the binder, and uniformly stirring at the rotating speed of 1000r/min to obtain the molybdenum disulfide coating. The preparation is carried out on the surface of an X80 matrix in a spraying mode, and the temperature is kept for 60min at 170 ℃ after the spraying. The sample was taken out and cooled to room temperature, and the thickness was 80 μm. The spraying process is to load the molybdenum disulfide coating into high-pressure airless spraying equipment and spray the molybdenum disulfide coating at the high pressure of 20 Mpa. Wherein the diameter of the molybdenum disulfide powder is 700nm, and the solid content of the molybdenum disulfide in the bottom layer is 47%.
And dispersing graphene oxide with the mass ratio of 0.1% in the slurry of the polytetrafluoroethylene, and stirring at the rotating speed of 950r/min for 20min to obtain the modified slurry of the polytetrafluoroethylene.
And after the bottom layer is completely dried, spraying modified polytetrafluoroethylene slurry, and baking for 80min in a muffle furnace at 170 ℃ to obtain the surface layer with the thickness of 85 microns. Wherein the spraying process comprises the steps of filling the slurry of the modified polytetrafluoroethylene into high-pressure airless spraying equipment, and spraying at the high pressure of 20 Mpa.
Comparative example 1
A novel composite hydrogen permeation resistant coating for pipeline steel was prepared using the method of example 2, except that no fluorine-containing coating was prepared.
Comparative example 2
A novel composite hydrogen permeation resistant coating for pipeline steel was prepared using the method of example 4, except that 0.1% graphene oxide was not added to the slurry of polytetrafluoroethylene.
Evaluation of Hydrogen permeation in examples 1 to 4 and comparative examples 1 to 2 was carried out by an electrochemical hydrogen permeation method, plating nickel on the uncoated side, at a current density of 5 to 50mA/cm 2 The time is 1-20min, the nickel plating solution adopts watt type nickel plating solution, a double-sided electrolytic cell is adopted, pt electrodes are used as auxiliary electrodes of an anode cell and a cathode cell, and the effective area of the Pt electrode plate is 1-10cm 2 Hg/HgO is used as a reference electrode of an anode pool, 0.2mol/L NaOH solution is added into the anode pool, and 1-3g/L thiourea is added into a cathode pool; setting the voltage of the anode pool at 0.15-0.2V relative to the reference electrode, introducing nitrogen for 0.5-1 h, and charging hydrogen with constant current of 10-100mA/cm into the cathode pool after the background current is stable 2 。
The hydrogen permeability coefficient was calculated using the following formula:
wherein D is the apparent hydrogen permeability coefficient, L is the thickness of the test sample, t L Is hydrogenTime of penetration current it =0.63i ∞
The electrochemical hydrogen permeability coefficient vs. ratio is shown in table 1.
TABLE 1 comparison of electrochemical hydrogen permeation coefficients of examples and comparative examples
According to the GB/T5210-2006 standard, the adhesion tests of examples 1-4 and comparative examples 1-2 are carried out by using a digital display pull-open method tester BGD500, and the impact resistance tests are carried out by using a paint film flexibility tester BGD 560 and a paint film impactor BGD 304. In the examples, the adhesive force is between 5 and 10Mpa, the impact strength is about 50Kg.cm, and the flexibility is 1mm.
And (3) carrying out full-tension and fatigue tests at normal temperature by adopting a hundreds-of-several PLW-50 50kN hydrogen environment electro-hydraulic servo fatigue testing machine, setting the stress amplitude to be 500Mpa, starting the test after hydrogen pre-charging for 24 hours, and recording the cycle frequency during fracture.
TABLE 2 cycle number at break of test
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention. It should be noted that other equivalent modifications can be made by those skilled in the art in light of the teachings of the present invention, and all such modifications can be made as are within the scope of the present invention.
Claims (12)
1. A composite hydrogen permeation resistant coating for a hydrogen transport pipeline, the coating comprising: the bottom layer is a molybdenum disulfide coating, and the surface layer is a modified fluorine-containing coating.
2. The composite hydrogen permeation resistant coating for the hydrogen transmission pipeline as claimed in claim 1, wherein the modified fluorine-containing coating is one or more of a modified polytetrafluoroethylene coating, a polyvinylidene fluoride coating and a fluorine-silicon coating.
3. The composite hydrogen permeation resistant coating for the hydrogen transmission pipeline as claimed in claim 1, wherein the solid content of molybdenum disulfide in the bottom layer is 38% -60%.
4. The composite hydrogen permeation resistant coating for the hydrogen transmission pipeline according to claim 1, wherein the thickness of the bottom layer is 20-80 μm, the thickness of the surface layer is 60-150 μm, and the total thickness of the composite hydrogen permeation resistant coating is 80-230 μm.
5. The composite hydrogen permeation resistant coating for the hydrogen transportation pipeline according to claim 1, wherein the hydrogen transportation pipeline is pipeline steel.
6. A method for preparing a composite hydrogen permeation resistant coating for a hydrogen transport pipeline as claimed in any one of claims 1 to 5, comprising:
(1) Preparation of the bottom layer: uniformly mixing molybdenum disulfide powder and a dispersing agent, and ultrasonically mixing and stirring for 20-60min to obtain a component A; adding a binder into the component A, uniformly stirring at the rotating speed of 600-1200r/min, heating to 55-80 ℃ in vacuum, and preserving heat for 60-300min to obtain a component B; the component B is blended into a diluent and added with a curing agent, and the mixture is uniformly stirred at the rotating speed of 800-1500r/min to obtain a molybdenum dioxide coating; spraying the molybdenum dioxide coating on the surface of the hydrogen conveying pipeline substrate, and keeping the temperature at 160-250 ℃ for 20-90min after spraying;
(2) Preparation of the surface layer: modifying the fluorine-containing coating by using graphene oxide, wherein the addition amount of the graphene oxide is 0.1-5%, and the dispersion is carried out for 10-60min at the rotating speed of 800-1500r/min to obtain the modified fluorine-containing coating; and (2) after the bottom layer prepared in the step (1) is completely dried, spraying the modified fluorine-containing coating on the surface of the bottom layer, and finally baking to form a stable surface layer.
7. The method according to claim 6, wherein the diameter of the molybdenum disulfide powder in step (1) is 100 to 800nm; the weight ratio of the molybdenum disulfide powder to the dispersant is 1:10-20 percent, the addition amount of the binder is 30-60 percent of the weight of the component A, and the mass ratio of the addition amount of the diluent to the component B is (1-3): 1, the addition amount of the curing agent is 10-30% of the weight of the binder.
8. The preparation method of claim 6, wherein the dispersant is one of acetone or ethanol containing 0.1-5% of a silane coupling agent, the binder is thermosetting polyurethane, the diluent is water, and the curing agent is isocyanate.
9. The preparation method according to claim 6, wherein the step (1) comprises grinding, degreasing and drying before spraying the molybdenum dioxide coating on the surface of the hydrogen pipeline substrate.
10. The method according to claim 6, wherein the bottom layer and the surface layer are prepared by spraying at a high pressure of 10-20Mpa using a high-pressure airless spraying device.
11. The preparation method according to claim 6, wherein the fluorine-containing coating is one or more of polytetrafluoroethylene, polyvinylidene fluoride and fluorine silicon.
12. The preparation method according to claim 6, wherein in the preparation process of the surface layer in the step (2), the baking process is carried out in a muffle furnace at the temperature of 150-300 ℃, and the surface layer is taken out and placed at room temperature after being kept for 20-90 min.
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